EP2495226B1 - Kompositgegenstand mit einer keramischen Nanokompositschicht - Google Patents
Kompositgegenstand mit einer keramischen Nanokompositschicht Download PDFInfo
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- EP2495226B1 EP2495226B1 EP11250237.2A EP11250237A EP2495226B1 EP 2495226 B1 EP2495226 B1 EP 2495226B1 EP 11250237 A EP11250237 A EP 11250237A EP 2495226 B1 EP2495226 B1 EP 2495226B1
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- European Patent Office
- Prior art keywords
- ceramic
- composite article
- recited
- nanocomposite layer
- oxide
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- 239000000919 ceramic Substances 0.000 title claims description 76
- 239000002114 nanocomposite Substances 0.000 title claims description 53
- 239000002131 composite material Substances 0.000 title claims description 31
- 239000000463 material Substances 0.000 claims description 30
- 229920000642 polymer Polymers 0.000 claims description 29
- 239000000758 substrate Substances 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims description 24
- 229910052751 metal Inorganic materials 0.000 claims description 22
- 239000002184 metal Substances 0.000 claims description 22
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 20
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 229910052796 boron Inorganic materials 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 229910021332 silicide Inorganic materials 0.000 claims description 10
- 229910052710 silicon Inorganic materials 0.000 claims description 10
- 239000010703 silicon Substances 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 9
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 8
- 229910052735 hafnium Inorganic materials 0.000 claims description 8
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 8
- 229910052726 zirconium Inorganic materials 0.000 claims description 8
- 150000002739 metals Chemical class 0.000 claims description 7
- 229910052715 tantalum Inorganic materials 0.000 claims description 7
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 7
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 7
- 229910052721 tungsten Inorganic materials 0.000 claims description 7
- 239000010937 tungsten Substances 0.000 claims description 7
- 229910052720 vanadium Inorganic materials 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 229910052758 niobium Inorganic materials 0.000 claims description 6
- 239000010955 niobium Substances 0.000 claims description 6
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 239000010936 titanium Substances 0.000 claims description 6
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 5
- 239000012700 ceramic precursor Substances 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 5
- 239000002243 precursor Substances 0.000 claims description 5
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 229910010293 ceramic material Inorganic materials 0.000 claims description 4
- 239000007769 metal material Substances 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 239000011733 molybdenum Substances 0.000 claims description 4
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 claims description 4
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 3
- -1 borides Inorganic materials 0.000 claims description 3
- 229910052702 rhenium Inorganic materials 0.000 claims description 3
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052582 BN Inorganic materials 0.000 claims description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 2
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 239000011651 chromium Substances 0.000 claims description 2
- 229910052706 scandium Inorganic materials 0.000 claims description 2
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims description 2
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims 4
- 229910052580 B4C Inorganic materials 0.000 claims 1
- 229910010271 silicon carbide Inorganic materials 0.000 claims 1
- 239000010410 layer Substances 0.000 description 41
- 230000001590 oxidative effect Effects 0.000 description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 150000001875 compounds Chemical group 0.000 description 4
- 238000000197 pyrolysis Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 229910000601 superalloy Inorganic materials 0.000 description 3
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 239000011153 ceramic matrix composite Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 150000002902 organometallic compounds Chemical class 0.000 description 2
- 238000010094 polymer processing Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 229910000531 Co alloy Inorganic materials 0.000 description 1
- 229940123973 Oxygen scavenger Drugs 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- DZPJVKXUWVWEAD-UHFFFAOYSA-N [C].[N].[Si] Chemical compound [C].[N].[Si] DZPJVKXUWVWEAD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001639 boron compounds Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000004320 controlled atmosphere Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005227 gel permeation chromatography Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- 239000012704 polymeric precursor Substances 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
- C04B41/5062—Borides, Nitrides or Silicides
- C04B41/5066—Silicon nitride
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/563—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on boron carbide
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
- C04B35/571—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained from Si-containing polymer precursors or organosilicon monomers
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
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- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23C18/1216—Metal oxides
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/122—Inorganic polymers, e.g. silanes, polysilazanes, polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1229—Composition of the substrate
- C23C18/1245—Inorganic substrates other than metallic
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
- C04B2235/483—Si-containing organic compounds, e.g. silicone resins, (poly)silanes, (poly)siloxanes or (poly)silazanes
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- C04B2235/486—Boron containing organic compounds, e.g. borazine, borane or boranyl
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D13/00—Electrophoretic coating characterised by the process
- C25D13/02—Electrophoretic coating characterised by the process with inorganic material
Definitions
- This disclosure relates to composite articles having a ceramic protective layer for improved thermal and oxidative protection.
- Ceramic and metallic materials are attractive materials for use in articles that operate under severe environmental conditions.
- gas turbine engine components are subjected to high temperatures, corrosive and oxidative conditions, and elevated stress levels.
- various types of barrier layers have been used to protect the underlying substrate from the elevated temperature conditions or corrosive/oxidative environment.
- Exemplary prior art layers and coatings are disclosed, for example, in US 5194338 , US 5558908 , US 5196059 and A.M. Tsirlin et al., Ceram. Eng. Sci. Proc. 23, 269 (2002 ).
- the present invention provides a composite article comprising: a substrate; and a ceramic nanocomposite layer disposed on the substrate, the ceramic nanocomposite layer comprising a pyrolized single-source polyborosilazane pre-ceramic polymer that is a single polymer precursor structure, rather than a mixture of two or more ceramic precursor sources, the ceramic nanocomposite layer having an amorphous microstructure with regions of ordered crystalline phases that have crystal grain dimensions or domains of less than one hundred nanometers, and the ceramic nanocomposite layer having a composition comprising silicon, boron, carbon and nitrogen, and at least one oxide-forming material selected from a group consisting of oxide-forming metals/semi-metals, borides, silicides, and combinations thereof, wherein the composition of the ceramic nanocomposite layer includes a ratio, R, of silicon atoms to boron atoms of 3 ⁇ R ⁇ 1.
- the present invention provides a method of processing a composite article, comprising: forming a ceramic nanocomposite layer by pyrolizing a single-source polyborosilazane pre-ceramic polymer that is a single polymer precursor structure, rather than a mixture of two or more ceramic precursor sources, such that the ceramic nanocomposite layer has an amorphous microstructure with regions of ordered crystalline phases that have crystal grain dimensions or domains of less than one hundred nanometers, and the ceramic nanocomposite layer having a composition that includes silicon, boron, carbon and nitrogen, and at least one oxide-forming material selected from a group consisting of oxide-forming metals/semi-metal borides, silicides, and combinations thereof on a substrate, wherein the composition of the ceramic nanocomposite layer includes a ratio, R, of silicon atoms to boron atoms of 3 ⁇ R ⁇ 1.
- Figure 1 illustrates selected portions of an example composite article 20 having improved thermal and oxidative stability, for example.
- the composite article 20 is not limited to any particular type and may be, for example only, a turbine engine blade or vane, a leading edge of an airfoil, a support structure in a turbine engine, a combustor can or liner, a seal, joint or joining article, a rocket component, other component over which hot exhaust gasses pass or other type of aerospace component.
- the composite article 20 may be for any type of application that would benefit from thermal and/or oxidative stability.
- the composite article 20 includes a substrate 22 and a ceramic nanocomposite layer 24 disposed on the substrate 22.
- the ceramic nanocomposite layer 24 protects the underlying substrate 22 from a high temperature environment and/or corrosive and oxidative environmental conditions.
- the ceramic nanocomposite layer 24 may be a coating on the substrate 22 or a matrix of a ceramic matrix composite
- the substrate 22 may be a fiber in a ceramic matrix composite, the body of a component, a barrier layer that is disposed on the body of a component, a matrix in which the nanocomposite layer 24 is disposed, or any other type of substrate that would benefit from the ceramic nanocomposite layer 24.
- the substrate 22 may be a silicon-based ceramic material or a metallic material.
- the silicon-based ceramic material may be silicon carbide (SiC), silicon nitride (Si 3 N 4 ), silicon carbonitride, a silicon-carbon-nitrogen-containing ceramic material, or combinations thereof, including oxygen-containing forms of these materials.
- the substrate 22 may be a metallic material, such as a superalloy.
- the superalloy may be a nickel-based or cobalt-based alloy.
- the substrate 22 would benefit from additional thermal and corrosion/oxidative resistance for the intended end use.
- the ceramic nanocomposite layer 24 facilitates improving the thermal and oxidative stability of the composite article 20.
- the ceramic nanocomposite layer 24 includes a composition having silicon, boron, carbon and nitrogen.
- the term "nanocomposite” may refer to a multi-phase microstructure wherein one or more of the phases includes at least one dimension that is less than one-hundred nanometers.
- the ceramic nanocomposite layer 24 may have more than one phase or all of its phases include at least one dimension that is less than one-hundred nanometers.
- the ceramic nanocomposite layer 24 may have all of the dimensions of each phase be less than one-hundred nanometers.
- nanocomposite or “nanophase” in this disclosure is also used to refer to materials that are considered amorphous, as determined by standard X-ray diffraction techniques, yet actually contain regions of ordered, crystalline phases with crystal grain dimensions or domains less than one-hundred nanometers.
- the particular nanophases of the ceramic nanocomposite layer 24 depend upon the processing methods used to form a ceramic nanocomposite layer 24.
- the ceramic nanocomposite layer 24 may include silicon nitride (Si 3 N 4 ) and boron nitride (BN).
- the boron nitride may be present in crystalline, amorphous or turbostratic forms.
- the ceramic nanocomposite layer 24 may also include carbon in the composition.
- the carbon may be present within the microstructure in various forms, such as silicon carbide (SiC), boron carbide (B 4 C) or as regions of graphite, turbostratic carbon or graphene.
- the composition of the ceramic nanocomposite layer 24 is controlled during processing by controlling a ratio, R, of silicon atoms to boron atoms.
- the ratio, R, of silicon atoms to boron atoms is 3 ⁇ R ⁇ 1.
- the ratio and processing parameters may be varied and controlled to yield particular compositions and microstructures that are beneficial for the intended end use application.
- Figure 2 illustrates an embodiment composite article 120 that is somewhat similar to the composite article 20 shown in Figure 1 .
- like reference numerals designate like elements where appropriate, and reference numerals with the addition of one hundred or multiples thereof designate modified elements that are understood to incorporate the same features and benefits of the corresponding original elements.
- the composite article 120 includes a ceramic nanocomposite layer 124 disposed on the substrate 22.
- the ceramic nanocomposite layer 124 is identical to the ceramic nanocomposite layer 24 but additionally includes an oxide-forming material 126 dispersed therethrough.
- the oxide-forming material 126 may include an oxide-forming metal or semi-metal selected from aluminum, titanium, zirconium, hafnium, vanadium, niobium, tantalum, chromium, boron, molybdenum, tungsten, yttrium, ytterbium, scandium, rhenium, and combinations thereof.
- the oxide-forming material 126 may be in elemental form or in compound form. In one example, the oxide-forming material 126 includes at least hafnium. In other examples, the oxide-forming material 126 includes at least zirconium and/or aluminum.
- the oxide-forming material 126 serves as an oxygen scavenger by reacting with available oxygen to form a stable oxide.
- the reaction with oxygen consumes at least a portion of the available oxygen and thereby prevents the oxygen from reacting with elements of the substrate 22 or elements of any other adjacent materials.
- the example oxides are thermally stable and may physically expand to self-repair microcracks in the ceramic nanocomposite layer 124.
- the oxides may also react with elements of the substrate 22 or elements from any adjacent materials to form stable compounds or glasses that further enhance the thermal stability of the composite article 120.
- the oxide-forming material 126 may additionally or alternatively include a boride material.
- the boride material may include at least one boride of titanium, zirconium, hafnium, niobium, vanadium, tantalum and tungsten.
- the borides are thermally stable and may react with elements of the substrate 22 or oxygen or elements from any adjacent materials to form stable compounds or glasses that further enhance the thermal stability of the composite article 120.
- the oxide-forming material 126 may additionally or alternatively include a silicide material.
- the silicide material may include at least one silicide of zirconium, hafnium, niobium, vanadium, titanium, tantalum, boron, molybdenum and tungsten.
- the silicides are thermally stable and may react with elements of the substrate 22 or oxygen or elements from any adjacent materials to form stable compounds or glasses that further enhance the thermal stability of the composite structure 120.
- An embodiment method of fabricating or processing the composite article 120 includes forming the ceramic nanocomposite layer 124 on the substrate 22. That is, the substrate 22 may be pre-fabricated and the ceramic nanocomposite layer 124 may be formed on the pre-fabricated substrate 22.
- the particular technique selected for forming the ceramic nanocomposite layer 124 may depend upon the type of substrate 22, the desired end properties of the composite article 120 or a desire to use a certain process.
- pre-ceramic polymer processing is used. Given this description, one of ordinary skill in the art will be able to recognize advantageous processing methods and parameters to meet their particular needs.
- the forming of the ceramic nanocomposite layer 24 includes pre-ceramic polymer processing to achieve atomic level mixing of the constituent elements in appropriate ratios.
- the process includes pyrolyzing a single-source pre-ceramic polymer in a controlled atmosphere such as nitrogen.
- the single-source pre-ceramic polymer is a polyborosilazane with the desired ratio, R, of silicon atoms to boron atoms. That is, the single-source is a single polymeric precursor structure rather than a mixture of two or more pre-ceramic precursor sources with the desired ratio, R, of silicon atoms to boron atoms.
- the pyrolysis may be conducted in a known manner, and the pre-ceramic polymer may be prepared in a known manner via reaction between organosilicon compounds and boron compounds.
- the ceramic nanocomposite layer 124 includes the oxide-forming material 126.
- the selected oxide-forming material or materials 126 along with any other additives are incorporated during the processing such that the final ceramic nanocomposite layer 124 includes the oxide-forming material or materials 126 and other additives.
- the metal or metals may be incorporated in metallic form by mixing with the pre-ceramic polymer prior to pyrolysis.
- the metal or metals may be provided as organometallic compounds that are mixed with the pre-ceramic polymer or precursors thereto.
- the metal or metals may be chemically incorporated into the polymer backbone of the pre-ceramic polymer rather than being physically mixed with the polymer.
- the borides or silicides may be incorporated in the pre-ceramic polymer prior to pyrolysis.
- solvents to improve dispersion of the oxide-forming material 126 is also contemplated. That is, the pre-ceramic polymer or the organometallic compound may be dissolved in a suitable solvent and mixed to ensure uniform distribution of the components. Following removal of the solvent through controlled heating and/or reduced pressure, a uniform mixture containing pre-ceramic polymer and oxide-forming material 126 is obtained.
- the single source pre-ceramic polymer provides the benefit of an atomic level mixture of the elements of the composition of the ceramic nanocomposite layer 124.
- the elements chemically bonded in the pre-ceramic polymer can remain following pyrolysis to form nanosized phases or domains, rather than micro- or macro-sized phases that collectively have lower thermal/oxidative stability or other disadvantageous properties.
- the single-source pre-ceramic polymer can be pyrolyzed at temperatures below 1200°C (2192 °F), which reduces thermal influence on the substrate 22. Higher temperatures may also be used to increase nanocrystal size or nanophase domain size or the extent of crystallinity of the phases, but may result in microstructures having less desirable phases or a substantial loss of boron or other elements of the composition.
- the ratio of silicon atoms to boron atoms may be controlled during the preparation of the pre-ceramic polymer to yield a final composition having a desired composition and properties. That is, the ratio of silicon atoms to boron atoms in the pre-ceramic polymer corresponds to the ratio in the final ceramic nanocomposite layer 124. Additionally, the silicon to boron ratio used in preparation of the polyborosilazane pre-ceramic polymer may control the molecular weight of the pre-ceramic polymer to tailor the polymer to certain processes.
- the pre-ceramic polymer with the above exemplary ratios may be further characterized by its molecular weight range, which may be between 1000-500,000 atomic mass units or Daltons as measured by standard gel permeation chromatography methods.
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Claims (14)
- Kompositgegenstand (120), umfassend:ein Substrat (22); undeine keramische Nanokompositschicht (124), die auf dem Substrat angeordnet ist, wobei die keramische Nanokompositschicht ein pyrolisiertes vorkeramisches Polyborsilazan-Polymer einer einzigen Quelle umfasst, das einer einzigen Polymervorläuferstruktur anstelle eines Gemischs von zwei oder mehr keramischen Vorläuferquellen entspricht, wobei die keramische Nanokompositschicht eine amorphe Mikrostruktur mit Regionen von geordneten kristallinen Phasen aufweist, die Kristallkornabmessungen oder -bereiche von unter hundert Nanometern aufweisen, und die keramische Nanokompositschicht eine Zusammensetzung, umfassend Silicium, Bor, Kohlenstoff und Stickstoff, und mindestens ein Oxid bildendes Material (126), ausgewählt aus einer Gruppe, bestehend aus Oxid bildenden Metallen/Halbmetallen, Boriden, Siliciden und Kombinationen davon, aufweist,wobei die Zusammensetzung der keramischen Nanokompositschicht ein Verhältnis, R, von Siliciumatomen zu Boratomen von 3 ≥ R ≥ 1 einschließt.
- Kompositgegenstand nach Anspruch 1, wobei die keramische Nanokompositschicht Siliciumnitrid und Bornitrid einschließt.
- Kompositgegenstand nach Anspruch 2, wobei der Kohlenstoff in Form von Siliciumcarbid, Borcarbid oder Kombinationen davon vorliegt.
- Kompositgegenstand nach einem der vorhergehenden Ansprüche, wobei das Oxid bildende Metall aus einer Gruppe ausgewählt ist, bestehend aus Aluminium, Titan, Zirconium, Hafnium, Vanadium, Niob, Tantal, Chrom, Molybdän, Wolfram, Yttrium, Ytterbium, Scandium, Rhenium und Kombinationen davon.
- Kompositgegenstand nach Anspruch 4, wobei das Oxid bildende Metall aus einer Gruppe ausgewählt ist, bestehend aus Vanadium, Tantal, Wolfram, Rhenium und Kombinationen davon.
- Kompositgegenstand nach Anspruch 4, wobei das Oxid bildende Metall Hafnium einschließt.
- Kompositgegenstand nach Anspruch 4, wobei das Oxid bildende Metall Zirconium einschließt.
- Kompositgegenstand nach Anspruch 4, wobei das Oxid bildende Metall Aluminium einschließt.
- Kompositgegenstand nach einem der vorhergehenden Ansprüche, wobei das Borid mindestens ein Metall einschließt, ausgewählt aus einer Gruppe, bestehend aus Titan, Zirconium, Hafnium, Niob, Vanadium, Tantal und Wolfram.
- Kompositgegenstand nach einem der vorhergehenden Ansprüche, wobei das Silicid mindestens ein Element einschließt, ausgewählt aus einer Gruppe, bestehend aus Zirconium, Hafnium, Niob, Vanadium, Titan, Tantal, Bor, Molybdän und Wolfram.
- Kompositgegenstand nach einem der vorhergehenden Ansprüche, wobei das Substrat ein keramisches Material auf Siliciumbasis oder ein metallisches Material ist.
- Verfahren zum Bearbeiten eines Kompositgegenstands (120), umfassend:Bilden einer keramischen Nanokompositschicht (124) durch das Pyrolisieren eines vorkeramischen Polyborsilazan-Polymers einer einzigen Quelle, das einer einzigen Polymervorläuferstruktur anstelle eines Gemischs von zwei oder mehr keramischen Vorläuferquellen entspricht, sodass die keramische Nanokompositschicht eine amorphe Mikrostruktur mit Regionen von geordneten kristallinen Phasen aufweist, die Kristallkornabmessungen oder -bereiche von unter hundert Nanometern aufweisen, und die keramische Nanokompositschicht eine Zusammensetzung, die Silicium, Bor, Kohlenstoff und Stickstoff aufweist, und mindestens ein Oxid bildendes Material (126), ausgewählt aus einer Gruppe, bestehend aus Oxid bildenden Metallen/Halbmetallen, Boriden, Siliciden und Kombinationen davon auf einem Substrat (22), aufweist,wobei die Zusammensetzung der keramischen Nanokompositschicht ein Verhältnis, R, von Siliciumatomen zu Boratomen von 3 ≥ R ≥ 1 einschließt.
- Verfahren nach Anspruch 12, wobei das Bilden der keramischen Nanokompositschicht bei einer Temperatur unterhalb von 1200 °C ausgeführt wird.
- Verfahren nach Anspruch 12 oder 13, wobei das Bilden der keramischen Nanokompositschicht das Verwenden eines vorkeramischen Polymers einschließt, das ein Molekulargewicht von 1.000-500.000 atomaren Masseneinheiten aufweist.
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